Artificial leather and process of making the same.



"UNITED snares PATENT @FFIGE.

LEON LILIENFELD, 0F VIENNA, AUSTRIA-HUNGARY.

. ARTIFICIAL LEATHER AND PROCESS OF MAKING THE SAME.

income.

Specification of Letters Patent.

Patented May 118, 11915.

No Drawing. Original application filed December 11, 1912, Serial No. 736,222. Divided and this application A filed July 11, 1914.

To all whom it may concern:

Be it known that I, Dr. LEON LILIEN-IELD,

chemist, a subject of the Emperor of Austria-Hungary, residing at No. 1 Zeltgasse,

. 5 'Vienna, VIII, in the Empire of Austria- Hungary, have invented certain new and useful Improvements in Processes for the Manufacture of Artificial Leather, as will be hereinafter fully described.

The present invention relates to a new and improved process for the manufacture of artificial leather and the like and product of Whichthe following is a specification.

Oils and fats and their derivatives and more especially castor oil, have chiefly been iised as agents for imparting softness and elasticity in the manufacture of artificial leather from colloided cellulose ester masses.

Said oils and fats and more especially castor oil have a great number ofdisadvantages, such as to impart an unpleasant smell to the artificial leather, to be of limited durability, small resistance to heat and the like. A very important disadvantage is that an alternate arrangement of layers of colloided cellulose ester p masses and viscose (cellulose xanthogenate) is not possible when oils and fats, and more especially castor oil, are employed as softening agents because such layers do not adhere to viscose, and Vice Versa.

The present invention is now based upon the fact that layers consisting of a matter of composition containing colloided cellulose ester masses and phenol esters which remain liquid at a temperature of 0 C. have a good adhes1on to layers of viscose and especially to layers of viscose mixed with products which are obtained by n treating aromatic amins with drying oils,

especially Chinese wood oil in the presence of condensing agentspas described in my U. S. Letters Patent No. 1037158 and further that layers of viscose mixed withsaid .5 products adhere likewise very well to layers consisting of colloided cellulose ester masses and the said phenol esters. One object of the present invention is therefore a new and improved process for o the manufacture of artificial leather and.

the like which consists in coating suitable materials with layers of a composition of matter containing a colloided cellulose ester mass and oneor more phenol esters which 5 remain liquid at a temperature of 0 C. al-

Serial No. amass.

ternating with layers composed of a mixture of viscose (cellulose xanthogenate) and the products obtained by treating drying oils, especially Chinese wood oil with aromatic amins in the presence of condensing agents.

Artificial leather and imitation wax cloth composed of layers of a colloided cellulose ester mass and phenol esters which remain liquid at 0 C., alternating with layers consisting of mixtures ofviscose and products obtained by heating aromatic amins with drying oils, especially Chinese wood oil and a condensing agent, are products valuable in the art, and are distinguished by their softness, pliability and gloss, and also cheapness,

In carrying out the improved process nitrocellulose or celluloid or substitutes therefor in general any cellulose esters are dissolved in a suitable solvent, and to the solution there is added a phenol ester which v remains liquid at 0 C. Ortho-tricresyl-phosphate has been found especially suitable for this purpose. This solution may. be also unixed with other suitable binding agents (for instance, acetyl-cellulose, formyl-cellulose, caoutchouc, guttapercha, drying oils coats orlayers. If the composition is applied in several layers the percentage either of nitrocellulose 0r celluloid or of phenol esters which remain liquid at 0 C. or of both may vary in any of the several layers.

Since the cellulose esters when only mixed with the said phenol esters and Well kneaded yield compositions or pastes capablea'of being applied or rolled on, there is no need to use volatile solvents, or if such are used the quantity used may be very small. The production of the crude or purlfied viscose is supposed to be known.

Themixtures of viscose with the products obtained from .Chinese wood oil, aromatic amins and a condensing agent are prepared by mixing by stirring and kneading together crude viscose or viscose refined by any known means (for instance by treatment with common salt or sal ammoniac or ammonium sulfate or other salts, or carbonic acid or alcohols or sodium bisulfite'or sulfurous acid, or weak acids or other dehydrating agents, etc.) or a dissolved heavy metal salt of vicose (for instance a zinc compound of viscose which is soluble in alkalis or ammonia) with the products obtained from Chinese wood oil, aromatic amins and a condensing agent.

'It has been found advantageous to prepare this mixture by adding the products of the Chinese wood oil and aromatic amins in the dissolved state to the viscose.

A'solution or emulsion of such products prepared with the help of basic substances (alkalis, ammonia and the like), soaps or alkali salts or ammonium salts of the fatty sulfoaci'ds (Turkey red oil, turkon oil 'and the like) and water, is especially suitable for this purpose.

The mixture of viscose with the product of Chinese wood oil and aromatic amins is then applied, with or'Without an admixture of coloring matters or pigments or filling substances (such as ground leather, finely powdered'cork, asbestos, zinc white, precipitated chalk, etc.) and with or without other binding agents (such as glue,. albumen, caoutch-ouc, resin, drying oils, etc.) or softening agents (such as lycerin, sugar, soaps, oils, etc.) in layers a ternating with layers of the composition composed of a colloided cellulose ester mass and phenol esters which remain liquid at 0 C. upon suitable materials (such as fabrics, paper and the like) by hand or machinery.

After drying, the artificial leather thus made is either leftto mature by storage for the purpose of rendering the viscose insoluble, or it is treated with substances that render viscose, insoluble or it is exposed to steam or to dry heat. If viscose still containing impurities has been used, a final washing process is needed, consisting in treating the artlficial leather either with wateralone or with water and acids.

The improved process'may, however, also be carried out by coating the material with the mixture of viscose and the product of Chinese wood oil and aromatic amins, rendering the viscose insoluble and freeing it from impurities and drying it in a known manner and then applyin the layers or the 1 mixture of a colloided 'ce lulose ester mass and the at 0 C.

The artificial leather thus produced may be satined or calendered either in layers or when finished. The completely finished artificial leather may be pressed or embossedphenol esters which remain liquid .weight of alcohol, 12 parts by weight of powdered celluloid, 12 parts by weight of ortho-tricresylphosphate.

Standard emulsion N 0. weight of .a substance produced by. heating 100 parts by weight of Chinese wood oil with 200 parts by Weight of ortho-toluidin and 11 parts by weight of zinc chlorid, washing in water and drying, are, while being stirred and kneaded together, heated to water bath temperature, and then 550 parts p .30 31-1000 parts by I by weight of soda-Turkey-red-oil of about 40 to 55 per cent. of dry residue and 6 to 10 per cent. of ash are added in several doses. Then 60 parts by weight of a soda solution of 50 B, are added .in several doses, and finally themass is diluted by kneading with 800 parts by weight of water. The finished solution or emulsion may th be strained for the purpose of freeing it rom impurities. Standard solutionv N o. 4.'-100 parts. by

weight of standard emulsion No. 3 are well mixed with 40 to '50 parts by weight'of a raw viscose containing 13 per cent. of cellulose.

Standard solution N 0. 5-100 parts by weight of standard emulsion No. 3 are well mixed with 7 5 to 100parts by weight ,of a raw viscose containing 13 per cent. of cellulose.

ios

Artificial leather No.1.A first layer con: 9

sisting of one to six coats of the standard solution No. 4 or No. 5 with the addition of a pigment, 'a pigment-lake or a coloring matter is applied upon a suitable material such as a. textile fabric and a second layer consisting of one to three coats of the standard solutions No. 1 .or No.- 2 are applied thereupon. When quite dry, the imitation leather is treated with hydrochloric or sulfuric acid of 5 to 10 per cent. stren h, then thoroughly washed and again drie Artificial leather N o. 2.'A first layer consisting of one to six coats of the" standard solution No. 4 or No. 5 is applied to a textile fabric or the like. After drying the artificial leather is'treated with steam or with a "mineral acid of 5 to 'lOper cent. strength and thoroughly washed and dried, whereupon a second layer consisting of one to three coats 1s given with the standard solution No. 1 or No.

Artificial leather N 0. 3.The same is made by applying four layers as follows: 1st layer (consisting of one to four coats) standard solution No. 4 or No. 5, 2nd layer (consisting of one to three coats) standard.

solution No. 1 or No. 2, 3rd layer (consisting of one to three coats) standard solution No. 4 or N o. 5, 4th layer (consisting of one to three coats) standard solution No. 1 or Since this imitation leather contains viscose, it must also be treated either with steam or with a mineral acid or the like, and then washed.

The artificial leathers may be calender-ed or pressed at the finish or between the several layers and finally marked with any desired leather graining or other design.

hat I claim as my invention and desire to secure by Letters Patent is:

1. The process for the manufacture of artificial leather and the like, which consists in coating suitable materials-with layerscomposed ofa colloided cellulose ester mass and a phenol ester which remains liquid at a temperature of 0 Cent. alternating with layers composed of a mixture of viscose (cellulose-xanthogenate) and the products obtained from Chinese wood oil and aromatic amins in the presence of a condensing agent.

2. The process for the manufacture of artificial leather and the like, which consists in coating suitable materials with layerscomposed of a mixture of a colloided ester mass, a phenol ester which remains liquid at a temperature of 0 Cent. and a solvent common to both, alternating with layers composed ofa mixture of viscose (cellulose xanthogenate) and the products obtained from Chinese wood oil and aromatio amins in the presence of a condensing as a softening agent, further softening;

agents, binding agents, filling substances and coloring matters, alternating with layers composed of a mixture of viscose (cellulose xanthogenate) and the products obtained from Chinesewood oil and aromatic amins in the presence of a condensing agent.

4. The process for the manufacture of artificial leather and the like, which consists in coating suitable materials with layers composed of a mixture of a colloided cellulose ester mass and orthotricresylphosphate alternating with layers composed of a mixture of viscose (cellulose xanthogenate) and the products obtained from Chinese wood oil and aromatic amins in the presence of a condensing agent.

5. As a new product artificial leather comprising a fabric coated with layers of a mixture ofia colloided cellulose ester mass.

and a phenol ester which remains liquid at 0 Cent. alternating with layers composed of a mixture of viscose (cellulose xanthogenate) and the products obtained from Chinese wood oils and aromatic amins in the presence of a condensing agent.

In testimony whereof I have signed my nameto this specification in the presence of two subscribing witnesses.

DR. LEON LILIENFELD. Witnesses:

HERMAN WUNDERLIGH, AUGUST FU'GGER. 

